CN100574792C - A kind of effective ingredient detection method of Chinese medicine composition - Google Patents
A kind of effective ingredient detection method of Chinese medicine composition Download PDFInfo
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Abstract
The invention discloses a kind of Chinese medicine composition, belong to the field of Chinese medicines.This Chinese medicine composition is to be got by certain prepared by a certain proportion of Flos Lonicerae, Radix Scutellariae, Herba Taraxaci, Herba Violae, Spina Gleditsiae, Radix Paeoniae Rubra, Caulis Spatholobi, rhizoma sparganic, Rhizoma Chuanxiong, Rhizoma Cyperi, Rhizoma Corydalis and Semen Vaccariae, and female pelvic inflammation is had better therapeutical effect.The present invention also discloses the preparation method and the method for quality control of this Chinese medicine composition.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition for the treatment of women's chronic pelvic inflammatory disease and preparation method thereof and method of quality control, belong to the field of Chinese medicines.
Background technology
Women's chronic pelvic inflammatory disease disease is commonly encountered diseases and the frequently-occurring disease in the gynaecopathia, causes very big misery to the patient, the object of the present invention is to provide a kind of evident in efficacy, the Chinese medicine composition of the treatment women's chronic pelvic inflammatory disease that has no side effect of taking convenience.
Summary of the invention
The present invention seeks to be achieved through the following technical solutions
Medicine of the present invention is made by following component:
Flos Lonicerae 15-25 part Radix Scutellariae 15-25 part Herba Taraxaci 10-20 part
5 parts-15 parts Spina Gleditsiae 10-20 part Radix Paeoniae Rubra of Herba Violae 10-20 part
5 parts-15 parts of 5 parts of-15 parts of Rhizoma Chuanxiongs of Caulis Spatholobi 15-25 part rhizoma sparganic
5 parts-15 parts of 5 parts of-15 parts of Semen Vaccariae of 5 parts of-15 parts of Rhizoma Corydalis of Rhizoma Cyperi
Medicine optimum weight part proportioning of the present invention is:
15 parts of 20 parts of Herba Taraxacis of 20 parts of Radix Scutellariaes of Flos Lonicerae
15 parts of 15 parts of Radix Paeoniae Rubra of 10 parts of Spina Gleditsiaes of Herba Violae
10 parts of 10 parts of Rhizoma Chuanxiongs of 20 parts of rhizoma sparganic of Caulis Spatholobi
10 parts of 10 parts of Semen Vaccariae of 10 parts of Rhizoma Corydalis of Rhizoma Cyperi
In the above crude drug, Rhizoma Cyperi and Rhizoma Corydalis are good with the vinegar goods, and Semen Vaccariae is good with parched medicinal material then.
Use above crude drug, can make acceptable various regular dosage forms on clinical or the pharmaceutics, comprise tablet, capsule, granule, soft capsule and pill etc.
Accomplish above dosage form, can pass through following processing step:
Two of purpose of the present invention can realize by following technical measures:
Get crude drug, pulverize, decoct with water secondary, collecting decoction filters, and filtrate is concentrated into clear paste, and stirring slowly adds ethanol down, fully stirs, and leaves standstill, and the leaching supernatant reclaims ethanol to clear paste, gets Chinese medicine composition; This Chinese medicine composition is added suitable adjuvant, make required dosage form.Such as:
Add disintegrating agent, binding agent, granulate, add volatile oil, add lubricant, be pressed into tablet.
Add disintegrating agent, binding agent, granulate, add volatile oil, add lubricant, incapsulate, make capsule.
Add substrate, suspending agent, wetting agent, be prepared into soft capsule.
Add distilled water, static, supernatant is got in cold preservation 24 hours, filters, and adds sedan-chair flavor agent and/or cosolvent and/or antiseptic, is prepared into oral solution.
Add sedan-chair flavor agent and excipient, be prepared into granule.
In detail, its preparation process is:
Get crude drug, decoct with water secondary, add 10 times of water gagings for the first time, decocted 2 hours, and added 6 times of water gagings for the second time, decocted 1 hour, collecting decoction, filter, relative density was 1.20～1.25 clear paste when filtrate was concentrated into 80 ℃, added ethanol and made and contain the alcohol amount and reach 50%, left standstill 24 hours, the leaching supernatant reclaims ethanol and is condensed into clear paste, gets Chinese medicine composition; Add in the drug composition hereinto distilled water and correctives and/antiseptic, make oral liquid.
In the process of this Chinese medicine composition of research, the inventor also formulates and has used some method of quality control, and these methods can be estimated the quality of control product.This method of quality control comprises assay and qualitative identification two parts, below narration respectively.
Content assaying method can adopt following method according to the needs of different dosage form:
A, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 10: 90～15: 85 acetonitrile-0.4% phosphoric acid solution is a mobile phase; The detection wavelength is 327 ± 2nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 1000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorogenic acid reference substance, puts in the brown measuring bottle, adds 50% methanol and make the solution that every 1ml contains 40-60 μ g, that is, preserve below 10 ℃;
It is an amount of that this product is got in the preparation of need testing solution, puts in the tool plug conical flask, adds 50% methanol 25-100ml, weigh, and supersound extraction 20-40 minute, add 50% methanol and supply the weight that subtracts mistake, filter, promptly;
Accurate reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid respectively, measures, promptly;
B, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, 45: 55: 0.1～50: 50: 0.2 methanol-water-phosphoric acid is a mobile phase, the detection wavelength is 280 ± 2nm, and theoretical cam curve is pressed the baicalin peak and calculated, and should be not less than 2500;
It is an amount of that the preparation precision of reference substance solution takes by weighing 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure, adds methanol and make the solution that every 1ml contains 40-60 μ g;
It is an amount of that this product is got in the preparation of need testing solution, and accurate the title decides, and the accurate methanol 25-100ml that adds claims to decide weight, and supersound process 20-40 minute, claim to decide weight, add methanol and supply the weight that subtracts mistake, filtration, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;
C, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 10: 90～20: 80 acetonitrile-0.1 phosphoric acid is mobile phase, detects wavelength 230 ± 2nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of that the preparation precision of the preparation reference substance solution of reference substance solution takes by weighing in phosphorus pentoxide desiccator 36 hours peoniflorin reference substance of drying under reduced pressure, adds mobile phase and make the solution that contains 40-60 μ g among every 1ml, shakes up, promptly;
It is an amount of that this product is got in the preparation of need testing solution, and accurate the title decides, and the accurate methanol 25-100ml that adds claims to decide weight, and supersound process 20-40 minute, claim again to decide weight, add methanol and supply the weight that subtracts mistake, filtration, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
Discrimination method then comprises following one or more:
A, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add water 20-50ml, and put hot bath and make dissolving, with n-butanol extraction 2-3 time, each 10-25ml, merging n-butyl alcohol liquid, water bath method, residue add an amount of methanol makes dissolving, as need testing solution; Other gets baicalin, chlorogenic acid reference substance, adds methanol respectively and makes the solution that every 1ml contains 0.1mg, in contrast product solution; According to the thin layer chromatography test, draw each 2-5 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp 365nm and inspect; For looking in the product chromatograph, with baicalin, the corresponding position of chlorogenic acid reference substance chromatograph on, the fluorescence speckle of apparent same color respectively;
B, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add water 20-50ml, and put hot bath and make dissolving, with n-butanol extraction 2-3 time, each 10-25ml, merging n-butyl alcohol liquid, water bath method, residue add an amount of methanol makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 50-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 40: 15: 10: chloroform-ethyl acetate of 0.2-methanol-formic acid was developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, be identical bluish violet speckle;
C, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add methanol 20-50ml supersound process 20-40 minute, filter, filtrate evaporate to dryness, residue add water makes dissolving, adds ammonia solution and transfers to alkalescence, ether extraction 2-3 time, each 10-25ml, merge extractive liquid,, evaporate to dryness, residue adds an amount of methanol makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 5-10 μ l, reference substance solution 1 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 10: 6: 1 cyclohexane extraction, one chloroform-methanol is developing solvent, launch, take out, dry, after putting in the iodine vapor smoked several seconds kind, put under the ultra-violet lamp 365nm and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
D, to get this product an amount of, solution elder generation evaporate to dryness, other dosage forms directly add water 20-50ml, with the dilute hydrochloric acid adjust pH to 2-3, hot bath makes dissolving, put cold, with ether extraction 2-3 time, each 10-25ml merges ether solution, extracts 2-3 time with 2% sodium carbonate liquor, each 10-25ml divides and gets alkali liquor, adds hydrochloric acid and regulates pH value to 2-3, add diethyl ether and extract 2-3 time, each 10-25ml merges ether solution, volatilize, residue adds an amount of methanol makes dissolving, as need testing solution; Other gets the ferulic acid reference substance and adds methanol and make the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 5-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-glacial acetic acid of 30: 1: 3-methanol is developing solvent, launches, and takes out, dry, under ultra-violet lamp 365nm, inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
This product can be used for women's chronic pelvic inflammatory disease card and belongs to damp-heat accumulation, and the auxiliary treatment of people who gets stagnation of vital energy and blood stasis for determining drug effect, has been carried out pharmacodynamics test research to this product, and used medicine is best proportioning and optimum process preparation and get according to the present invention in the test.
Concrete test is as follows:
Test an external bacteriostasis
Adopting golden yellow glucose coccus, staphylococcus epidermidis is test strain.
Test method: adopt agar dilution.With making doubling dilution in the agar culture medium that be added in by the reagent thing to have melted, pour into the plating medium that becomes to contain different liquor strengths.With the method for reduced turbidity, each bacterial strain is diluted to 1/2 of No. 1 standard pipe in Maxwell, dibbling is on the plating medium of variable concentrations respectively for the bacterium liquid that dilution is good, and every 10 μ l cultivated 18～24 hours for 37 ℃.Be provided with the contrast of blank and penicillin positive drug simultaneously.Write down the growing state of each bacterial strain on different pharmaceutical concentration culture medium, the least concentration that this medicine suppresses bacteria growing is minimal inhibitory concentration, and minimal inhibitory concentration (MIC) expression bacteriostatic level is adopted in this test.
Result of the test shows that this product oral solutions has the vitro inhibition effect to golden Portugal bacterium and form staph.Result of the test sees Table 1.
The external bacteriostasis of table 1 is table as a result
| Test strain | Bacterial strain number (strain) | The antibacterial contrast | Penicillin contrast (100U/ml) | MIC scope (mg/ml) |
| Gold The Portugal bacterium | 20 | + | - | 20.6～100 |
| Table The Portugal bacterium | 20 | + | - | 15.5～100 |
Test the influence of two xylol induced mice auricle edemas
Experimental technique faces with preceding that this product granule is mixed with the 0.10gPml suspension with 0.5% Carboxymethyl cellulose sodium (CMC-Na) is standby, and animal is used healthy Kunming mouse, body weight 20 ± 2 grams.Mice is divided into five groups (matched group normal saline) at random, irritate the long-pending 20mlPkg of being of body of stomach, two weeks of continuous irrigation stomach, once a day, the last administration was applied to mouse right ear with microsyringe with 0.05mlP dimethylbenzene after 30 minutes, put to death mice after 15 minutes, cut two ears along the auricle baseline, dash with the 8mm diameter steel and to lay round auricle in left and right sides auricle same area respectively, torsion balance claims two auricle weight in wet bases,, calculate and respectively organize swelling degree average and standard deviation as the swelling level index with two auricle weight differences, carry out the t check.Inhibitory rate of intumesce equals the difference of average swelling degree of matched group and the average swelling degree of administration group and takes advantage of 100% again divided by the average swelling degree of matched group.
The results are shown in Table 2, the result shows that two dosage groups of this product granule and matched group compare, and auricle swelling degree obviously alleviates, and significant differences is arranged, and illustrates that this product has good antiinflammatory action.
Table 2 xylol
Induced miceThe influence of auricle edema
Annotate: matched group is * P＜0.05 relatively, * * P＜0.01
Further specify technical scheme of the present invention by the following examples, but the present invention to protect preparation be not limited in the described dosage form of embodiment.
The specific embodiment:
Embodiment 1
[prescription] Flos Lonicerae 200g Radix Scutellariae 200g Herba Taraxaci 150g
Herba Violae 100g Spina Gleditsiae 150g Radix Paeoniae Rubra 150g
Caulis Spatholobi 200g rhizoma sparganic 100g Rhizoma Chuanxiong 100g
Rhizoma Cyperi (vinegar system) 100g Rhizoma Corydalis (vinegar system) 100g Semen Vaccariae (stir-fry) 100g
[method for making] above 12 flavors are given as one thinks fit cataclasmly, decoct with water secondary, for the first time add 10 times of water gagings, decocted 2 hours, add 6 times of water gagings for the second time, decocted 1 hour, collecting decoction filters, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (80 ℃), stir and slowly to add ethanol down and make and contain the alcohol amount and reach 50%, fully stir, left standstill 24 hours, the leaching supernatant reclaims the clear paste of ethanol to relative density 1.30～1.35 (80 ℃).Get 1 part of clear paste, 3 parts of sucrose, 1 part in dextrin and ethanol are an amount of, granulate, and drying is made 1000g, promptly.
Embodiment 2
[prescription] Flos Lonicerae 250g Radix Scutellariae 250g Herba Taraxaci 200g
Herba Violae 150g Spina Gleditsiae 200g Radix Paeoniae Rubra 200g
Caulis Spatholobi 250g rhizoma sparganic 150g Rhizoma Chuanxiong 150g
Rhizoma Cyperi 150g Rhizoma Corydalis 150g Semen Vaccariae 150g
[method for making] gets crude drug, decocts with water secondary, adds 10 times of water gagings for the first time, decocted 2 hours, and added 6 times of water gagings for the second time, decocted 1 hour, collecting decoction filters, and relative density was 1.20～1.25 clear paste when filtrate was concentrated into 80 ℃, add ethanol and make and contain the alcohol amount and reach 50%, left standstill the leaching supernatant 24 hours, reclaim ethanol and be condensed into clear paste, add a small amount of ethyl hydroxybenzoate, and adding distil water gets oral liquid to 1000ml.
Granule carries out quality examination among embodiment 3 embodiment
This product 5g is got in [discriminating] (1), adds water 50ml, puts hot bath and makes dissolving, uses n-butanol extraction 2 times, and each 20ml merges n-butyl alcohol liquid, and water bath method, residue add 2ml methanol makes dissolving, as need testing solution.Other gets baicalin, chlorogenic acid reference substance, adds methanol respectively and makes the solution that every 1ml contains 0.1mg, in contrast product solution.According to the thin layer chromatography test, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.For looking in the product chromatograph, with baicalin, the corresponding position of chlorogenic acid reference substance chromatograph on, the fluorescence speckle of apparent same color respectively.
(2) get the peoniflorin reference substance, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw reference substance solution and discriminating (1) item each 10 μ l of need testing solution down, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-methanol-formic acid (40: 15: 10: 0.2) be developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, be identical bluish violet speckle.
(3) get this product 5g, porphyrize adds methanol 50ml supersound process 30 minutes, filters the filtrate evaporate to dryness, residue adds water makes dissolving, adds ammonia solution and transfers to alkalescence, ether extraction 3 times, each 15ml, merge extractive liquid,, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 1 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with cyclohexane extraction one chloroform-methanol (10: 6: 1) is developing solvent, launch, take out, dry, after putting in the iodine vapor smoked several seconds kind, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(4) get this product 10g, add water 50ml, with dilute hydrochloric acid adjust pH to 2～3, hot bath makes dissolving, put cold, with ether extraction 3 times, each 20ml merges ether solution, extracts 3 times with 2% sodium carbonate liquor, each 15ml divides and gets alkali liquor, adds hydrochloric acid and regulates pH value to 2～3, add diethyl ether and extract 3 times, each 15ml merges ether solution, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the ferulic acid reference substance and adds methanol and make the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-glacial acetic acid-methanol (30: 1: 3) is developing solvent, launches, and takes out, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
[assay] is according to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.4% phosphoric acid solution (13: 87) is a mobile phase; The detection wavelength is 327nm.Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 1000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorogenic acid reference substance, puts in the brown measuring bottle, adds 50% methanol and make the solution that every 1ml contains 40 μ g, promptly gets (preserving below 10 ℃).
This product is got in the preparation of need testing solution, porphyrize, and precision takes by weighing 5g, put in the tool plug conical flask, add 50% methanol 30ml, supersound extraction 25 minutes, filter, residue is with 50% washed with methanol 3 times, 5ml at every turn, filter, merging filtrate quantitatively shifts in the 100ml measuring bottle, adds 50% methanol and is diluted to scale, shake up, promptly.
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid respectively, measure, promptly.
The every 10g of this product contains chlorogenic acid (C16H1809) must not be less than 7.0mg.
Claims (2)
1. the effective ingredient detection method of a Chinese medicine composition, its raw material of Chinese medicine consists of: Flos Lonicerae 15-25 part, Radix Scutellariae 15-25 part Herba Taraxaci 10-20 part, Herba Violae 5-15 part, Spina Gleditsiae 10-20 part, Radix Paeoniae Rubra 10-20 part, Caulis Spatholobi 15-25 part, rhizoma sparganic, 5-15 part, Rhizoma Chuanxiong 5-15 part, Rhizoma Cyperi 5-15 part, Rhizoma Corydalis 5-15 part, Semen Vaccariae 5-15 part; It is characterized in that this method comprises one or more of following content assaying method:
A, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 10: 90～15: 85 acetonitrile-0.4% phosphoric acid solution is a mobile phase; The detection wavelength is 327 ± 2nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 1000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorogenic acid reference substance, puts in the brown measuring bottle, adds 50% methanol and make the solution that every 1ml contains 40-60 μ g, that is, preserve below 10 ℃;
It is an amount of that this product is got in the preparation of need testing solution, puts in the tool plug conical flask, adds 50% methanol 25-100ml, weigh, and supersound extraction 20-40 minute, add 50% methanol and supply the weight that subtracts mistake, filter, promptly;
Accurate reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid respectively, measures, promptly;
B, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, 45: 55: 0.1～50: 50: 0.2 methanol-water-phosphoric acid is a mobile phase, the detection wavelength is 280 ± 2nm, and theoretical cam curve is pressed the baicalin peak and calculated, and should be not less than 2500;
It is an amount of that the preparation precision of reference substance solution takes by weighing 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure, adds methanol and make the solution that every 1ml contains 40-60 μ g;
It is an amount of that this product is got in the preparation of need testing solution, and accurate the title decides, and the accurate methanol 25-100ml that adds claims to decide weight, and supersound process 20-40 minute, claim to decide weight, add methanol and supply the weight that subtracts mistake, filtration, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;
C, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 10: 90～20: 80 acetonitrile-0.1 phosphoric acid is mobile phase, detects wavelength 230 ± 2nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of that the preparation precision of the preparation reference substance solution of reference substance solution takes by weighing in phosphorus pentoxide desiccator 36 hours peoniflorin reference substance of drying under reduced pressure, adds mobile phase and make the solution that contains 40-60 μ g among every 1ml, shakes up, promptly;
It is an amount of that this product is got in the preparation of need testing solution, and accurate the title decides, and the accurate methanol 25-100ml that adds claims to decide weight, and supersound process 20-40 minute, claim again to decide weight, add methanol and supply the weight that subtracts mistake, filtration, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
2. detection method according to claim 1 is characterized in that this method comprises one or more in the following discrimination method:
A, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add water 20-50ml, and put hot bath and make dissolving, with n-butanol extraction 2-3 time, each 10-25ml, merging n-butyl alcohol liquid, water bath method, residue add an amount of methanol makes dissolving, as need testing solution; Other gets baicalin, chlorogenic acid reference substance, adds methanol respectively and makes the solution that every 1ml contains 0.1mg, in contrast product solution; According to the thin layer chromatography test, draw each 2-5 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp 365nm and inspect; For looking in the product chromatograph, with baicalin, the corresponding position of chlorogenic acid reference substance chromatograph on, the fluorescence speckle of apparent same color respectively;
B, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add water 20-50ml, and put hot bath and make dissolving, with n-butanol extraction 2-3 time, each 10-25ml, merging n-butyl alcohol liquid, water bath method, residue add an amount of methanol makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 50-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 40: 15: 10: chloroform-ethyl acetate of 0.2-methanol-formic acid was developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, be identical bluish violet speckle;
C, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add methanol 20-50ml supersound process 20-40 minute, filter, filtrate evaporate to dryness, residue add water makes dissolving, adds ammonia solution and transfers to alkalescence, ether extraction 2-3 time, each 10-25ml, merge extractive liquid,, evaporate to dryness, residue adds an amount of methanol makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 5-10 μ l, reference substance solution 1 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with cyclohexane extraction-chloroform-methanols of 10: 6: 1 was developing solvent, launch, take out, dry, after putting in the iodine vapor smoked several seconds kind, put under the ultra-violet lamp 365nm and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
D, to get this product an amount of, solution elder generation evaporate to dryness, other dosage forms directly add water 20-50ml, with the dilute hydrochloric acid adjust pH to 2-3, hot bath makes dissolving, put cold, with ether extraction 2-3 time, each 10-25ml merges ether solution, extracts 2-3 time with 2% sodium carbonate liquor, each 10-25ml divides and gets alkali liquor, adds hydrochloric acid and regulates pH value to 2-3, add diethyl ether and extract 2-3 time, each 10-25ml merges ether solution, volatilize, residue adds an amount of methanol makes dissolving, as need testing solution; Other gets the ferulic acid reference substance and adds methanol and make the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 5-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-glacial acetic acid of 30: 1: 3-methanol is developing solvent, launches, and takes out, dry, under ultra-violet lamp 365nm, inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
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| CN101019981B (en) * | 2007-03-15 | 2011-08-17 | 北京同御康泰科技有限公司 | Chinese medicine preparation and its preparing process |
| CN101849999B (en) * | 2009-03-31 | 2012-05-23 | 江苏康缘药业股份有限公司 | Chinese medicinal composition for treating pelvic inflammation and preparation method thereof |
| CN101940745B (en) * | 2010-09-07 | 2012-01-18 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating particles and preparation method thereof |
| CN101940746B (en) * | 2010-09-10 | 2012-05-23 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating pills and preparation method thereof |
| CN102973731A (en) * | 2011-09-05 | 2013-03-20 | 王成光 | Pelvic inflammatory disease and dysmenorrheal treatment liquid agent and preparation method thereof |
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